HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-methyl-5-methylthio-11H-1,2,4-triazolo[2,3-c][1,3]benzodiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 5-Methyl-3-(o-isothiocyanatobenzyl)-1,2,4-triazole | HCID 23317336 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-methyl-5-methylthio-11H-1,2,4-triazolo[2,3-c][1,3]benzodiazepine | HCID 23317318 | — |
Reaction Steps
To a suspension of 0.91 g of sodium hydride in 27 ml of tetrahydrofuran is added dropwise a solution of 8.74 g of 5-methyl-3-(o-isothiocyanatobenzyl)-1,2,4-triazole in 60 ml of tetrahydrofuran over a period of 20 minutes. The mixture is stirred at room temperature for 2 hours. To the resulting suspension is added a solution of 5.4 g of methyl iodide in 35 ml of tetrahydrofuran dropwise at 0° over a period of 15 minutes. The mixture is stirred at room temperature for 1 hour, poured into water and extracted three times with methylene chloride. The organic extracts are dried over magnesium sulfate, decolorized with charcoal and evaporated to give 2-methyl-5-methylthio-11H-1,2,4-triazolo[2,3-c][1,3]benzodiazepine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04595535 |
| Source dataset | uspto-grants-1986_06 |
| ORD ID | ord-5f5ba15bfab2406fa119bd1f7b997984 |
| Source note | uspto-grants-1986_06 |